CN101734630A - Method for preparing high-purity cadmium telluride - Google Patents
Method for preparing high-purity cadmium telluride Download PDFInfo
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- CN101734630A CN101734630A CN200910312590A CN200910312590A CN101734630A CN 101734630 A CN101734630 A CN 101734630A CN 200910312590 A CN200910312590 A CN 200910312590A CN 200910312590 A CN200910312590 A CN 200910312590A CN 101734630 A CN101734630 A CN 101734630A
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Abstract
The invention discloses a method for preparing high-purity cadmium telluride. The reaction process is carried out in a closed quartz tube with melting point above cadmium and tellurium and after carbon coating treatment, wherein the mass ratio of a 5N cadmium material to a 5N tellurium material is 1: 1.1-1.15. The method comprises the following steps: dividing the weighed tellurium material into N parts according to the charging times N, dividing the weighed cadmium material into N-1 parts, alternately adding each part of tellurium material and each part of cadmium material into the quartz tube and adding the tellurium material into the quartz tube firstly and lastly, removing oxygen after charging, sintering and sealing the tube by using a sealed bulb, and slowly performing high-temperature and high-pressure synthetic reaction. The method has the advantages that the contact area of the raw materials is larger in a molten state, the reaction speed is more sufficient compared with the solid raw material, the micro-sized crushing treatment for the raw materials is avoided, the shape requirement of the raw materials is relaxed, the preparation cost is greatly reduced, the purity of the raw material is ensured, the method is suitable for large-scale production, the synthetic conversion rate of the cadmium telluride can reach 98 to 99.5 percent, and the single-tube yield of 800 to 1,000 grams can be ensured by using the quartz tube with the inside diameter of 32 millimeters under the premise of safety.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity cadmium telluride, especially a kind of preparation method that need not carry out the high-purity cadmium telluride more than abrasive dust is handled, reaction process occurs in cadmium and tellurium the fusing point to raw material.
Background technology
Cadmium telluride is a kind of compound semiconductor, and its energy gap width is suitable for photovoltaic energy conversion most.The solar cell made from this semi-conductor is a kind of luminous energy to be converted into the device of electric energy, and very high theoretical light photoelectric transformation efficiency is arranged.Cadmium telluride can be made into large-area Cadimium telluride thin film with vapour deposition process, and deposition is also high.Just because of the cadmium telluride diaphragm solar battery low cost of manufacture, and have high conversion rate, add that therefore it can be fit to large solar module commercialization volume production in rapid large-area deposition under the hot environment.
Up to now, some very fruitful effort have appearred in the research about high-purity cadmium telluride, a kind of preparation method of high-purity cadmium telluride is disclosed as Chinese patent 200710049890.5, be characterized in 5N tellurium and 1: 1 in molar ratio proportioning of 5N cadmium are mixed, pellet is pulverized or ground to form to compound, particle diameter is 8～13 μ m, 500～600 weight parts, pack in the silica tube, be evacuated to 1～1.2pa sealing, again the silica tube behind the good seal put into the cadmium telluride synthetic furnace and react, this technology is that raw material is made particulate, increase the contact area of two kinds of raw materials with this, at the fusing point of cadmium with synthetic cadmium telluride down.Whole process can not produce bigger vapour pressure, and cadmium can not react with silica tube yet.But, the weak point of its existence is: the pellet that particle diameter is 8～13 μ m need be pulverized or grind to form to (1) compound, need the support of higher-end equipment, it is special because cadmium belongs to the soft metal, abrasive dust is difficulty very, grind micron-sized particle near the sky-high price cost, incompatible practical situation of producing.(2) in the process of carrying out material pulverizing, be difficult to avoid the pollution of equipment to raw material, can not prepare 6N even more high-grade cadmium telluride.
Another part Chinese patent 02114571.7 discloses a kind of preparation method of cadmium antimonide powder: at first cadmium powder and tellurium powder are mixed by stoicheiometry, mixed material is ground, stirs cadmium powder and tellurium powder are mixed; Mixed uniformly cadmium powder and tellurium powder are placed crucible under the vacuum condition, crucible is heated, make cadmium powder and tellurium powder in the crucible carry out combination reaction, form the cadmium telluride material; Adopt this invention can improve the purity of finished product significantly, and can not pollute and damage environment and operator, this technology be reacted under the fusing point of cadmium, has equally also avoided the reaction between vapour pressure and cadmium and the quartz.But weak point is: (1) this technology also is the powder preparation that feeds intake, and preparation powder stock cost height to the equipment requirements harshness, can cause the pollution to equipment.(2) the prepared product of this technology is only limited to the cadmium telluride particle, is difficult to guarantee aspect synthetic ratio.
In sum, those skilled in the art it has been generally acknowledged that the preparation of cadmium telluride should carry out below the fusing point of cadmium, and its advantage is: the whole process of reacting under the fusing point of cadmium can not produce bigger vapour pressure, and cadmium can not react with silica tube yet.Weak point is: (1) is in order to improve product purity, to improve synthetic ratio, the contact area that must increase raw material under the solid state reacts fully, therefore micron-sized pellet must be pulverized or ground to form to compound, the problem of bringing thus is the support that needs higher-end equipment, it is special because cadmium belongs to the soft metal, abrasive dust is difficulty very, grind micron-sized particle near the sky-high price cost, incompatible practical situation of producing.(2) in the process of carrying out material pulverizing, be difficult to avoid of the pollution of abrasive dust equipment to raw material, can not prepare highly purified cadmium telluride.(3) fusing point of cadmium is lower than tellurium, reacts under the fusing point of cadmium, and cadmium material and tellurium material are solid-state, and reaction is not as cadmium material and tellurium material sufficient reacting under the fused solution.
Avoid raw material is pulverized or milled processed and guarantee that simultaneously one of method that stock yard fully contacts is that raw material is reacted under molten state, those skilled in the art is not difficult to expect this scheme, and the inventor thinks that this scheme should carry out in airtight silica tube, should not in crucible, carry out, its reason is: crucible is synthetic to be to be based upon on the basis of material pulverizing, it is synthetic to have only abrasive dust to realize under the fusing point of tellurium and cadmium, and truly avoid steam, if synthesize at tellurium with more than the cadmium fusing point with crucible, have bigger raw material steam, on the crucible basis, make vacuum environment and need add seal closure, sealing difficulty is big, poor reliability, tightness is difficult to guarantee, in building-up process, can constantly there be steam to rise, steam with can condensation after the seal closure that is lower than vapor temperature all the time contacts attached on the seal closure, cause raw material to run off, synthetic ratio and purity all can't guarantee.Therefore should in airtight silica tube, synthesize, but the technical problem that this method needs to be resolved hurrily is: (1) is because the synthetic of cadmium telluride is thermopositive reaction, if synthesize more than the fusing point of raw material, a large amount of heat is emitted in reaction makes the silica tube internal pressure increase rapidly, bombing easily.(2) cadmium steam can react, influence product purity and synthetic ratio with silica tube.(3) difficult sealing under the high temperature high vacuum situation is to realize.These difficult problems all directly determine the synthetic success or failure even the personnel's of threat safety, therefore at present do not see have this method of successful Application to synthesize the relevant report of high-purity cadmium telluride method in batches.
Summary of the invention
The objective of the invention is to: provide a kind of and make the fully reaction in the airtight silica tube in deoxidation under the molten state of tellurium material and cadmium material, the raw material form is not had harsh require, high-purity cadmium telluride preparation method with low cost.
In order to solve the above-mentioned series technique problem that the sealed silica envelope internal reaction of raw material under molten state exists, the contriver has carried out exploring repeatedly in the invention process, has solved following technical problem:
1, synthetic vapour pressure is big
The synthetic existence form with tellurium and cadmium of cadmium telluride has much relations.Because the synthetic of cadmium telluride is thermopositive reaction, it is interior and not visible that whole process is in vacuum environment.Wherein, if the tellurium that drops into is Powdered, when vacuumizing, is pulled away easily, runs off.Otherwise, if the tellurium that drops into is excessive particle, because the fusing point of cadmium is low, at the beginning of heating up, the cadmium of liquid can generate cadmium telluride with the tellurium reaction that is contacted, with the most of tellurium parcel of the residue of macrobead tellurium material, when waiting to reach the fusing point of tellurium, remaining most of tellurium and the complete contact reacts of cadmium can be emitted a large amount of heat and be made the pipe internal pressure increase bombing easily rapidly.
Therefore, need raw material is handled before feeding intake, choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall, wash the zone of oxidation on surface then, it is stand-by that its surface is presented behind the white metal gloss; With the fragmentation of 5N tellurium material, make particle diameter stand-by in 0.35-20mm; Adopt the tellurium material of this particle diameter that higher surface area can be arranged, make reaction make two bites at a cherry, occur in the fusing point of cadmium and the fusing point of tellurium respectively.
The mode that feeds intake is: load weighted tellurium material is divided into N part according to reinforced times N, load weighted cadmium material is divided into N-1 part, every part of tellurium material and every part of cadmium material are alternately added through being coated with the silica tube that carbon handles and adding the tellurium material at first, add the tellurium material at last, N 〉=2 wherein, the benefit of doing like this is: make cadmium, tellurium uniform distribution, guarantee each instead would not be very violent; The tellurium material at two ends is wrapped up in intermediary cadmium material package, makes whole stockpile surface not have cadmium to expose, and guarantees can not form bigger cadmium steam before the first set reaction.
The silica tube that will unload from vacuum system is put into synthetic furnace, slowly be warming up to 600 ℃～800 ℃ with 100 ℃～200 ℃/hour speed, constant temperature 1.5～2.5 hours, the back slowly is warming up to 1100～1200 ℃ with 100～200 ℃/hour speed, constant temperature is 2.5～3.5 hours again, slowly be cooled to 900 ℃～1050 ℃ with 100-200 ℃/hour speed, the benefit of doing like this is: owing to invention feeds intake more relatively, there is the transmittance process of heat the inside of material, reaching fusing point also has the branch of priority, therefore in the temperature control process, heat up, make raw material melting reaction gradually with 100～200 ℃/hour slow speed; Slowly cooling is can be even for crystallization, reduces pore; The homothermic effect is to guarantee to synthesize fully.
2, cadmium steam and silica tube reaction
Directly contact with silica tube for fear of cadmium, be coated with the last layer carbon film at the silica tube inwall before the charging, technology abbreviates as and is coated with carbon: heating furnace temperature to 800～1100 ℃, silica tube is put the synthetic process furnace that is used for, fix ventpipe, feed the high-purity argon gas bubbling with 0.5～1 liter/minute speed and carry acetone steam to enter silica tube, acetone is subjected to form carbon film at the silica tube inwall after the thermo-cracking.Simultaneously, move the process furnace that is loaded with silica tube, can make carbon film even like this with the speed of 10～20cm/10 second.
More or less can contain oxide compound in the raw material, if the oxide compound in the raw material does not eliminate, not only can influence the purity of product, carbon film that also can oxidation silica tube inwall in building-up process causes carbon film to come off, and can not realize the isolation of cadmium and silica tube.Therefore, be necessary to carry out deoxidization technique and handle: behind the heating deoxidation stove to 200 ℃～280 ℃, silica tube is put into the vacuum system deoxidation, with the vacuum unit system is evacuated to high vacuum the oxide compound in the raw material is volatilized, when the vacuum tightness of vacuum system reaches 5 * 10
-4Pa～10 * 10
-4With the silica tube tube sealing, stop deoxidation behind the tube sealing behind the pa; Deoxidation temperature is crossed to hang down and can not be got a desired effect the too high easy loss cadmium of temperature.
3, the sealing of high temperature high vacuum
Owing to synthetic temperature height of the present invention, to the vacuum requirements height, can not use traditional rubber seal mode, therefore the contriver expects adopting the sealing of quartzy envelope bubble, vacuum system is made up of vacuum pump and diffusion pump, during vacuum deaeration, the position of material charging region 10～15cm places a quartzy envelope bubble in silica tube, and its external diameter is slightly less than the silica tube internal diameter.After vacuum deaeration is finished, with silica tube inwall and envelope bubble outer wall sintering, realize sealing to reaction zone with oxyhydrogen flame.
Deoxidation of the present invention, tube sealing requires the silica tube traverse, in order to adapt to deoxidation, the pipe sealing arts demand, consider that tube sealing needs the silica tube traverse, consider the weight that joint need bear silica tube and raw material, deoxidation temperature is not high, deoxidation finishes and can be easy to unload inferior factor, therefore, the contriver has designed a kind of high vacuum joint, its integral material is a stainless steel, in establish stainless steel lasso and rubbery loop, be arranged with screw thread outward, rely on the advance and retreat extruding of screw thread or loosen rubber case, realize the high vacuum sealing and unload silica tube, rubber cradle wherein, the stainless steel packing ring is arranged alternately, be enclosed within together on the silica tube that installs raw material with stainless steel outer sleeve, put into quartzy envelope bubble, be connected in the stainless steel and put, stainless steel outer sleeve is connected with external threading in the stainless steel, with rubber cradle, the extruding of stainless steel packing ring is tight, play the effect of sealing, treat deoxidation, tube sealing finishes, the vacuum system venting, move back screw thread by stainless steel outer sleeve, can unload stainless steel outer sleeve easily, and can change the stainless steel outer sleeve and the interior cover of stainless steel of different size according to different body sizes.
Therefore, the contriver has proposed following technical scheme:
A kind of preparation method of high-purity cadmium telluride, this method mainly may further comprise the steps:
(1) silica tube is coated with the carbon processing
In the silica tube of cleaning, adopt the pyrolytic reaction depositing carbon film;
(2) raw material is handled
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall, wash the zone of oxidation on surface, it is stand-by that its surface is presented behind the white metal gloss;
With the fragmentation of 5N tellurium material, make particle diameter stand-by in 0.35-20mm;
(3) batching
Weighing quality proportioning is 1: 1.1～1.15 5N cadmium material and 5N tellurium material;
(4) feed intake
Load weighted tellurium material is divided into N part according to reinforced times N, load weighted cadmium material is divided into N-1 part, every part of tellurium material and every part of cadmium material are alternately added through being coated with the silica tube that carbon handles and adding the tellurium material at first, add tellurium material, wherein N 〉=2 at last;
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 200 ℃～280 ℃, silica tube is put into the vacuum system deoxidation, when the vacuum tightness of vacuum system reaches 5 * 10
-4Pa～10 * 10
-4With the silica tube tube sealing, stop deoxidation behind the tube sealing behind the pa;
(6) building-up reactions
The silica tube that will unload from vacuum system is put into synthetic furnace, slowly be warming up to 600 ℃～800 ℃ with 100 ℃～200 ℃/hour speed, constant temperature 1.5～2.5 hours, the back slowly is warming up to 1100～1200 ℃ with 100～200 ℃/hour speed, constant temperature is 2.5～3.5 hours again, slowly is cooled to 900 ℃～1050 ℃ with 100-200 ℃/hour speed;
(7) get material
Break silica tube and take out the cadmium telluride product.
As optimal way, it is such before feeding intake silica tube being coated with the process that carbon handles: heating furnace temperature to 800～1100 ℃, fix ventpipe, feeding the high-purity argon gas bubbling with 0.5～1 liter/minute speed carries acetone steam to enter silica tube, simultaneously, the speed with 10～20cm/10 second moves the process furnace that is loaded with silica tube.
As optimal way, the process that described 5N cadmium material washes surface oxide layer is: the nitric acid and the alcohol mixeding liquid of preparation 5%～10%, soak 5N cadmium material, and 80 ℃～100 ℃ oven dry are cleaned to neutral after presenting white metal gloss in the surface with ethanol.
As optimal way, the process that described 5N cadmium material washes surface oxide layer is: the nitric acid and the alcohol mixeding liquid of preparation 5%～10%, soak 5N cadmium material, the surface is cleaned to neutral with ion exchanged water after presenting white metal gloss, uses vacuum drying oven 80 ℃～100 ℃ dryings.
As optimal way, described tube sealing process is: the envelope bubble is put into silica tube, be pushed into 10～15cm place, distance material district, will seal bubble and silica tube sintering tube sealing with oxyhydrogen flame.
As optimal way, silica tube to be put into vacuum system by the high vacuum interface carry out deoxidation, described high vacuum interface links into an integrated entity with silica tube, vacuum system respectively by screw thread.
Beneficial effect of the present invention is: (1) makes particle diameter in 0.35-20mm by before feeding intake the tellurium material being handled, the phenomenon of having avoided dusty raw materials when vacuumizing, to be pulled away easily, to run off, and higher surface area is arranged; If the tellurium material of oversized particles, because the fusing point of cadmium is low, at the beginning of heating up, the cadmium of liquid can generate cadmium telluride with the tellurium reaction that is contacted, with the most of tellurium parcel of the residue of macrobead tellurium material, when waiting to reach the fusing point of tellurium, remaining most of tellurium and the complete contact reacts of cadmium, can emit a large amount of heat makes the pipe internal pressure increase bombing easily rapidly.(2) every part of tellurium material and every part of cadmium material are alternately added silica tube and add the tellurium material at first, add the feeding mode of tellurium material at last, make cadmium, tellurium uniform distribution, guarantee each instead would not be very violent, the tellurium material at two ends is wrapped up in intermediary cadmium material package, make whole stockpile surface not have cadmium to expose, guarantee can not form bigger cadmium steam before the first set reaction.(3) because invention feeds intake more relatively, there is the transmittance process of heat the inside of material, reaching fusing point also has the branch of priority, therefore in the temperature control process, heat up with 100～200 ℃/hour slow speed, can make raw material thawing gradually abundant, slowly cooling be for crystallization can be even, reduce pore, the homothermic effect is to guarantee to synthesize fully.(4) be coated with the last layer carbon film at the silica tube inwall before the charging, avoided cadmium to contact, guaranteed synthetic ratio and purity with the direct of silica tube.(5) handle by deoxidization technique, removed the oxide compound in the raw material, guaranteed the purity of product, also avoided in building-up process the oxidation of silica tube inwall carbon film is guaranteed the isolation of cadmium and silica tube.(6) come sealed silica envelope by quartz envelope bubble, guarantee the requirement of synthetic high-temperature condition of high vacuum degree.(7) need not be again with raw material pulverizing or to grind to form particle diameter be micron-sized powder, simplified work flow, saved expensive that abrasive dust brings, avoided in the abrasive dust process equipment to the pollution of raw material, thereby guaranteed the purity of product, be beneficial to batch process.(8) cadmium telluride Synthesis conversion of the present invention can reach 98～99.5%, uses internal diameter 32mm silica tube can guarantee single tube output 800-1000g under the prerequisite of safety.(9) the raw material contact area under the molten state is bigger, and the raw material reaction speed under more solid-state is faster more abundant.
The GD-MS test data of the 5N high-purity cadmium telluride product that obtains sees Table 1.
Description of drawings
Fig. 1 is this preparation method's a schematic flow sheet
Fig. 2 is the synoptic diagram of tube sealing process among Fig. 1
Fig. 3 is the synoptic diagram that is coated with the carbon process among Fig. 1
Fig. 4 is the structural representation of the high vacuum joint among Fig. 2.
1 is quartzy envelope bubble, and 2 is raw material, and 3 is silica tube, 4 is vacuum system, and 5 is the high vacuum joint, and 6 are the deoxidation stove, 7 is ventpipe, and 8 is the bubbling bottle, and 9 is acetone, 10 is rubber cradle, and 11 is the stainless steel packing ring, and 12 is anchor, 13 is stainless steel outer sleeve, 14 is screw, and 15 is cover in the stainless steel, and 16 is the vacuum system mouth.
Embodiment
The preparation method of 1 first kind of high-purity cadmium telluride of embodiment may further comprise the steps:
(1) silica tube is coated with the carbon processing
As shown in Figure 3, when the furnace temperature for the treatment of deoxidation stove 6 reaches 800 ℃, fix ventpipe 7, feed argon gas, begin bubbling in the acetone 9, acetone steam is brought into ventpipe 7 with 0.5 liter/minute speed.Acetone comes out from ventpipe, and cracking under hot conditions simultaneously, is moved silica tube 3 after ventpipe or the cleaning with the speed of 10cm/10 second, adheres at quartzy tube wall to form one deck carbon film.
(2) raw material is handled
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall;
With the agate rod 5N tellurium raw material is smashed in the agate alms bowl, make particle diameter stand-by in 0.35～10mm; Sieve removes powder, with the tellurium material that screens out at H
2Melting crystal under the atmosphere is in order to using next time; The nitric acid and the alcohol mixeding liquid of preparation 5% soak 5N cadmium material, and 80 ℃ of oven dry are cleaned to neutral after presenting white metal gloss in the surface with ethanol.
(3) batching
Weighing 5N cadmium material 400 weight parts and 5N tellurium material 440 weight parts;
(4) feed intake
Load weighted tellurium material is divided into 3 parts, load weighted cadmium material is divided into 2 parts, respectively every part of raw material is fed into the silica tube that is coated with behind the carbon according to the sequencing of tellurium material, cadmium material, tellurium material, cadmium material, tellurium material;
The envelope bubble is put into silica tube, be pushed into 10cm place, distance material district, its external diameter is slightly less than the silica tube internal diameter;
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 200 ℃, silica tube is put into the vacuum system deoxidation, vacuum system 4 is made up of vacuum pump and diffusion pump, and silica tube is put into the high vacuum interface, tightens overcoat, drives vacuum pump, when the vacuum tightness of vacuum system reaches 5 * 10
-4To seal bubble 1 and silica tube 3 sintering tube sealings with oxyhydrogen flame behind the pa, realize sealing, as shown in Figure 2, stop vacuum pump behind the tube sealing reaction zone;
High vacuum joint 5 structures as shown in Figure 4, rubber cradle 10, stainless steel packing ring 11 are arranged alternately and stainless steel outer sleeve 13 is enclosed within on the silica tube 3 that installs raw material 2 together, put into quartzy envelope bubble 1, are connected in the stainless steel on the cover 15.Cover 15 is threaded in stainless steel outer sleeve 13 and the stainless steel, with rubber cradle 10,11 extruding of stainless steel packing ring tightly, plays the effect of sealing.Treat that deoxidation, tube sealing finish, the vacuum system venting is moved back screw thread by stainless steel outer sleeve 15, can unload stainless steel outer sleeve 13 easily.And can change the stainless steel outer sleeve 13 and the interior cover 15 of stainless steel of different size according to different body sizes.
(6) building-up reactions
The silica tube that will unload from vacuum system is checked vacuum tightness, put into synthetic furnace then, be warming up to 600 ℃ with 100 ℃/hour speed, 600 ℃ of constant temperature 1.5 hours, be warming up to 1200 ℃ with 100 ℃/hour speed, constant temperature is 2.5 hours again, and cooling has a power failure when being cooled to 900 ℃ with 100 ℃/hour.
(7) get material
Break silica tube with the titanium bar and take out the material ingot, remove the head flour, get 824 weight part cadmium tellurides.
The preparation method of 2: the second kinds of high-purity cadmium tellurides of embodiment may further comprise the steps:
(1) silica tube is coated with the carbon processing
As shown in Figure 3, when the furnace temperature for the treatment of deoxidation stove 6 reaches 1100 ℃, fix ventpipe 7, feed argon gas, begin bubbling in the acetone 9, acetone steam is brought into ventpipe 7 with 0.8 liter/minute speed.Acetone comes out from ventpipe, and cracking under hot conditions simultaneously, is moved silica tube 3 after ventpipe or the cleaning with the speed of 15cm/10 second, forms one deck carbon film at quartzy tube wall.
(2) raw material is handled
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall;
With the agate rod 5N tellurium raw material is smashed in the agate alms bowl, make particle diameter stand-by in 10～20mm; Sieve removes powder, with the tellurium material that screens out at H
2Melting crystal under the atmosphere is in order to using next time; The nitric acid and the alcohol mixeding liquid of preparation 10% soak 5N cadmium material, and 100 ℃ of oven dry are cleaned to neutral after presenting white metal gloss in the surface with ethanol.
(3) batching
Weighing 5N cadmium material 400 weight parts and 5N tellurium material 448 weight parts;
(4) feed intake
Load weighted tellurium material is divided into 2 parts, load weighted cadmium material as 1 part, is fed into every part of raw material the silica tube that is coated with behind the carbon respectively according to the sequencing of tellurium material, cadmium material, tellurium material;
The envelope bubble is put into silica tube, be pushed into 14cm place, distance material district, its external diameter is slightly less than the silica tube internal diameter.
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 240 ℃, silica tube is put into the vacuum system deoxidation, vacuum system 4 is made up of vacuum pump and diffusion pump, and silica tube is put into the high vacuum interface, tightens overcoat, drives vacuum pump, when the vacuum tightness of vacuum system reaches 8 * 10
-4To seal bubble 1 and silica tube 3 sintering tube sealings with oxyhydrogen flame behind the pa, realize sealing, as shown in Figure 2, stop vacuum pump behind the tube sealing reaction zone;
High vacuum joint 5 structures as shown in Figure 4, rubber cradle 10, stainless steel packing ring 11 are arranged alternately and stainless steel outer sleeve 13 is enclosed within on the silica tube 3 that installs raw material 2 together, put into quartzy envelope bubble 1, are connected in the stainless steel on the cover 15.Cover 15 is threaded in stainless steel outer sleeve 13 and the stainless steel, with rubber cradle 10,11 extruding of stainless steel packing ring tightly, plays the effect of sealing.Treat that deoxidation, tube sealing finish, the vacuum system venting is moved back screw thread by stainless steel outer sleeve 15, can unload stainless steel outer sleeve 13 easily.And can change the stainless steel outer sleeve 13 and the interior cover 15 of stainless steel of different size according to different body sizes.
(6) building-up reactions
The silica tube that will unload from vacuum system is checked vacuum tightness, put into synthetic furnace then, be warming up to 700 ℃ with 150 ℃/hour speed, 700 ℃ of constant temperature 2 hours, be warming up to 1100 ℃ with 150 ℃/hour speed, constant temperature is 3.5 hours again, and cooling has a power failure when being cooled to 1000 ℃ with 150 ℃/hour.
(7) get material
Break silica tube with the titanium bar and take out the material ingot, remove the head flour, get 839 weight part cadmium tellurides.
Embodiment 3: the preparation method of the third high-purity cadmium telluride may further comprise the steps:
(1) silica tube is coated with the carbon processing
As shown in Figure 3, when the furnace temperature for the treatment of deoxidation stove 6 reaches 900 ℃, fix ventpipe 7, feed argon gas, begin bubbling in the acetone 9, acetone steam is brought into ventpipe 7 with 1 liter/minute speed.Acetone comes out from ventpipe, and cracking under hot conditions simultaneously, is moved silica tube 3 after ventpipe or the cleaning with the speed of 20cm/10 second, forms one deck carbon film at quartzy tube wall.
(2) raw material is handled:
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall;
With the agate rod 5N tellurium raw material is smashed in the agate alms bowl, make particle diameter stand-by in 0.35～0.5mm; Sieve removes powder, with the tellurium material that screens out at H
2Melting crystal under the atmosphere is in order to using next time; Prepare 5% nitric acid and alcohol mixeding liquid, soak 5N cadmium material, the surface is cleaned to neutral with ion exchanged water after presenting white metal gloss, uses vacuum drying oven 80 ℃ of dryings.
(3) batching
Weighing 5N cadmium material 471 weight parts and 5N tellurium material 534 weight parts;
(4) feed intake
Load weighted tellurium material is divided into 4 parts, load weighted cadmium material is divided into 3 parts, respectively every part of raw material is fed into the silica tube that is coated with behind the carbon according to the sequencing of tellurium material, cadmium material, tellurium material, cadmium material, tellurium material, cadmium material, tellurium material;
The envelope bubble is put into silica tube, be pushed into 15cm place, distance material district, its external diameter is slightly less than the silica tube internal diameter.
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 280 ℃, silica tube is put into the vacuum system deoxidation, vacuum system 4 is made up of vacuum pump and diffusion pump, and silica tube is put into the high vacuum interface, tightens overcoat, drives vacuum pump, when the vacuum tightness of vacuum system reaches 10 * 10
-4To seal bubble 1 and silica tube 3 sintering tube sealings with oxyhydrogen flame behind the pa, realize sealing, as shown in Figure 2, stop vacuum pump behind the tube sealing reaction zone;
High vacuum joint 5 structures as shown in Figure 4, rubber cradle 10, stainless steel packing ring 11 are arranged alternately and stainless steel outer sleeve 13 is enclosed within on the silica tube 3 that installs raw material 2 together, put into quartzy envelope bubble 1, are connected in the stainless steel on the cover 15.Cover 15 is threaded in stainless steel outer sleeve 13 and the stainless steel, with rubber cradle 10,11 extruding of stainless steel packing ring tightly, plays the effect of sealing.Treat that deoxidation, tube sealing finish, the vacuum system venting is moved back screw thread by stainless steel outer sleeve 15, can unload stainless steel outer sleeve 13 easily.And can change the stainless steel outer sleeve 13 and the interior cover 15 of stainless steel of different size according to different body sizes.
(6) building-up reactions
The silica tube that will unload from vacuum system is checked vacuum tightness, put into synthetic furnace then, be warming up to 800 ℃ with 200 ℃/hour speed, 800 ℃ of constant temperature 2.5 hours, be warming up to 1150 ℃ with 200 ℃/hour speed, constant temperature is 3 hours again, and cooling has a power failure when being cooled to 1050 ℃ with 200 ℃/hour.
(7) get material
Break silica tube with the titanium bar and take out the material ingot, remove the head flour, get 1000 weight part cadmium tellurides.
The preparation method of 4: the four kinds of high-purity cadmium tellurides of embodiment may further comprise the steps:
(1) silica tube is coated with the carbon processing
As shown in Figure 3, when the furnace temperature for the treatment of deoxidation stove 6 reaches 1000 ℃, fix ventpipe 7, feed argon gas, begin bubbling in the acetone 9, acetone steam is brought into ventpipe 7 with 1 liter/minute speed.Acetone comes out from ventpipe, and cracking under hot conditions simultaneously, is moved silica tube 3 after ventpipe or the cleaning with the speed of 20cm/10 second, forms one deck carbon film at quartzy tube wall;
(2) raw material is handled:
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall;
With the agate rod 5N tellurium raw material is smashed in the agate alms bowl, make particle diameter stand-by in 0.5～2mm; Sieve removes powder, with the tellurium material that screens out at H
2Melting crystal under the atmosphere is in order to using next time; Prepare 10% nitric acid and alcohol mixeding liquid, soak 5N cadmium material, the surface is cleaned to neutral with ion exchanged water after presenting white metal gloss, uses vacuum drying oven 100 ℃ of dryings;
(3) batching
Weighing 5N cadmium material 400 weight parts and 5N tellurium material 456 weight parts;
(4) feed intake
Load weighted tellurium material is divided into 3 parts, load weighted cadmium material is divided into 2 parts, respectively every part of raw material is fed into the silica tube that is coated with behind the carbon according to the sequencing of tellurium material, cadmium material, tellurium material, cadmium material, tellurium material;
The envelope bubble is put into silica tube, be pushed into 14cm place, distance material district, its external diameter is slightly less than the silica tube internal diameter.
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 280 ℃, silica tube is put into the vacuum system deoxidation, vacuum system 4 is made up of vacuum pump and diffusion pump, and silica tube is put into the high vacuum interface, tightens overcoat, drives vacuum pump, when the vacuum tightness of vacuum system reaches 10 * 10
-4To seal bubble 1 and silica tube 3 sintering tube sealings with oxyhydrogen flame behind the pa, realize sealing reaction zone.As shown in Figure 2, stop vacuum pump behind the tube sealing;
High vacuum joint 5 structures as shown in Figure 4, rubber cradle 10, stainless steel packing ring 11 are arranged alternately and stainless steel outer sleeve 13 is enclosed within on the silica tube 3 that installs raw material 2 together, put into quartzy envelope bubble 1, are connected in the stainless steel on the cover 15.Cover 15 is threaded in stainless steel outer sleeve 13 and the stainless steel, with rubber cradle 10,11 extruding of stainless steel packing ring tightly, plays the effect of sealing.Treat that deoxidation, tube sealing finish, the vacuum system venting is moved back screw thread by stainless steel outer sleeve 15, can unload stainless steel outer sleeve 13 easily.And can change the stainless steel outer sleeve 13 and the interior cover 15 of stainless steel of different size according to different body sizes.
(6) building-up reactions
The silica tube that will unload from vacuum system is checked vacuum tightness, put into synthetic furnace then, be warming up to 800 ℃ with 200 ℃/hour speed, 800 ℃ of constant temperature 2 hours, be warming up to 1200 ℃ with 200 ℃/hour speed, constant temperature is 3.5 hours again, and cooling has a power failure when being cooled to 1050 ℃ with 200 ℃/hour.
(7) get material
Break silica tube with the titanium bar and take out the material ingot, remove the head flour, get 850 weight part cadmium tellurides.
The preparation method of 5: the five kinds of high-purity cadmium tellurides of embodiment may further comprise the steps:
(1) silica tube is coated with the carbon processing
As shown in Figure 3, when the furnace temperature for the treatment of deoxidation stove 6 reaches 1100 ℃, fix ventpipe 7, feed argon gas, begin bubbling in the acetone 9, acetone steam is brought into ventpipe 7 with 0.8 liter/minute speed.Acetone comes out from ventpipe, and cracking under hot conditions simultaneously, is moved silica tube 3 after ventpipe or the cleaning with the speed of 15cm/10 second, forms one deck carbon film at quartzy tube wall;
(2) raw material is handled:
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall;
With the agate rod 5N tellurium raw material is smashed in the agate alms bowl, make particle diameter stand-by in 0.35～20mm; Sieve removes powder, with the tellurium material melting crystal under H2 atmosphere that screens out, in order to using next time; The nitric acid and the alcohol mixeding liquid of preparation 8% soak 5N cadmium material, and 90 ℃ of oven dry are cleaned to neutral after presenting white metal gloss in the surface with ethanol.
(3) batching
Weighing 5N cadmium material 400 weight parts and 5N tellurium material 460 weight parts;
(4) feed intake
Load weighted tellurium material is divided into 4 parts, load weighted cadmium material is divided into 3 parts, respectively every part of raw material is fed into the silica tube that is coated with behind the carbon according to the sequencing of tellurium material, cadmium material, tellurium material, cadmium material, tellurium material, cadmium material, tellurium material;
The envelope bubble is put into silica tube, be pushed into 12cm place, distance material district, its external diameter is slightly less than the silica tube internal diameter.
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 240 ℃, silica tube is put into the vacuum system deoxidation, vacuum system 4 is made up of vacuum pump and diffusion pump, and silica tube is put into the high vacuum interface, tightens overcoat, drives vacuum pump, when the vacuum tightness of vacuum system reaches 8 * 10
-4To seal bubble 1 and silica tube 3 sintering tube sealings with oxyhydrogen flame behind the pa, realize sealing reaction zone.As shown in Figure 2, stop vacuum pump behind the tube sealing;
High vacuum joint 5 structures as shown in Figure 4, rubber cradle 10, stainless steel packing ring 11 are arranged alternately and stainless steel outer sleeve 13 is enclosed within on the silica tube 3 that installs raw material 2 together, put into quartzy envelope bubble 1, are connected in the stainless steel on the cover 15.Cover 15 is threaded in stainless steel outer sleeve 13 and the stainless steel, with rubber cradle 10,11 extruding of stainless steel packing ring tightly, plays the effect of sealing.Treat that deoxidation, tube sealing finish, the vacuum system venting is moved back screw thread by stainless steel outer sleeve 15, can unload stainless steel outer sleeve 13 easily.And can change the stainless steel outer sleeve 13 and the interior cover 15 of stainless steel of different size according to different body sizes.
(6) building-up reactions
The silica tube that will unload from vacuum system is checked vacuum tightness, put into synthetic furnace then, be warming up to 700 ℃ with 150 ℃/hour speed, 700 ℃ of constant temperature 2 hours, be warming up to 1160 ℃ with 150 ℃/hour speed, constant temperature is 3.5 hours again, and cooling has a power failure when being cooled to 1000 ℃ with 150 ℃/hour.
(7) get material
Break silica tube with the titanium bar and take out the material ingot, remove the head flour, get 851 weight part cadmium tellurides.
Table 1 5N high-purity cadmium telluride impurity element GD-MS test data (concentration: ppb)
| Si28(MR) | 539.9802 | 516.3564 | 504.5635 |
| Ca44(MR) | 19.8737 | 11.0141 | 6.7151 |
| Cr52(MR) | 1.4904 | 1.8512 | 1.4277 |
| Si28(MR) | 539.9802 | 516.3564 | 504.5635 |
| Fe56(MR) | 144.4963 | 109.4437 | 58.0333 |
| Ni60(MR) | 222.5717 | 235.2649 | 251.7308 |
| Cu63(MR) | 177.7133 | 98.1144 | 80.9804 |
| Zn66(MR) | 3.3865 | 2.215 | 2.9279 |
| As75(HR) | 3.2125 | 2.0334 | 3.0946 |
| Ag109(HR) | 9.4527 | 11.6302 | 9.2453 |
| Cd114(MR) | 441012303.9 | 439130141.2 | 438046721.9 |
| Cd114(HR) | 392691298.7 | 406847418.2 | 401984040.7 |
| Sn119(MR) | 1.0439 | 1.2385 | 0.2987 |
| Te130(MR) | 558951167 | 560833417 | 561916172.5 |
| Te130(HR) | 607269142.4 | 593113861.6 | 597975444.3 |
| Pb208(MR) | 135.9255 | 139.9378 | 143.3827 |
| Bi209(MR) | 6.2306 | 4.305 | 4.836 |
Claims (6)
1. the preparation method of a high-purity cadmium telluride is characterized in that this method mainly may further comprise the steps:
(1) silica tube is coated with the carbon processing
In the silica tube of cleaning, adopt the pyrolytic reaction depositing carbon film;
(2) raw material is handled
Choose the cadmium ingot of particle diameter less than the purity 5N of silica tube inwall, wash the zone of oxidation on surface then, it is stand-by that its surface is presented behind the white metal gloss;
Tellurium material fragmentation with purity 5N makes particle diameter stand-by in 0.35-20mm;
(3) batching
Weighing quality proportioning is 1: 1.1～1.15 5N cadmium material and 5N tellurium material;
(4) feed intake
Load weighted tellurium material is divided into N part according to reinforced times N, load weighted cadmium material is divided into N-1 part, every part of tellurium material and every part of cadmium material are alternately added through being coated with the silica tube that carbon handles and adding the tellurium material at first, add tellurium material, wherein N 〉=2 at last;
(5) deoxidation, tube sealing
Behind the heating deoxidation stove to 200 ℃～280 ℃, silica tube is put into the vacuum system deoxidation, after the vacuum tightness of vacuum system reaches 5 * 10-4pa～10 * 10-4pa,, stop deoxidation behind the tube sealing the silica tube tube sealing;
(6) building-up reactions
The silica tube that will unload from vacuum system is put into synthetic furnace, slowly be warming up to 600 ℃～800 ℃ with 100 ℃～200 ℃/hour speed, constant temperature 1.5～2.5 hours, the back slowly is warming up to 1100～1200 ℃ with 100～200 ℃/hour speed, constant temperature is 2.5～3.5 hours again, slowly is cooled to 900 ℃～1050 ℃ with 100-200 ℃/hour speed;
(7) get material
Break silica tube and take out the cadmium telluride product.
2. the preparation method of high-purity cadmium telluride according to claim 1, it is characterized in that, described silica tube is coated with carbon and handles and to be performed such: heating furnace temperature to 800～1100 ℃, fix ventpipe, feeding the high-purity argon gas bubbling with 0.5～1 liter/minute speed carries acetone steam to enter silica tube, simultaneously, the speed with 10～20cm/10 second moves the process furnace that is loaded with silica tube.
3. the preparation method of high-purity cadmium telluride according to claim 1, it is characterized in that, the process that described 5N cadmium material washes surface oxide layer is: the nitric acid and the alcohol mixeding liquid of preparation 5%～10%, soak 5N cadmium material, 80 ℃～100 ℃ oven dry are cleaned to neutral after presenting white metal gloss in the surface with ethanol.
4. the preparation method of high-purity cadmium telluride according to claim 1, it is characterized in that, the process that described 5N cadmium material washes surface oxide layer is: the nitric acid and the alcohol mixeding liquid of preparation 5%～10%, soak 5N cadmium material, the surface is cleaned to neutral with ion exchanged water after presenting white metal gloss, uses vacuum drying oven 80 ℃～100 ℃ dryings.
5. the preparation method of high-purity cadmium telluride according to claim 1 is characterized in that, described tube sealing process is: the envelope bubble is put into silica tube, be pushed into 10～15cm place, distance material district, will seal bubble and silica tube sintering tube sealing with oxyhydrogen flame.
6. the preparation method of high-purity cadmium telluride according to claim 1 is characterized in that: silica tube is put into vacuum system by the high vacuum interface carry out deoxidation, described high vacuum interface links into an integrated entity with silica tube, vacuum system respectively by screw thread.
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